CN107475552A - A kind of preparation method of silver-nickel material - Google Patents
A kind of preparation method of silver-nickel material Download PDFInfo
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- CN107475552A CN107475552A CN201710687107.1A CN201710687107A CN107475552A CN 107475552 A CN107475552 A CN 107475552A CN 201710687107 A CN201710687107 A CN 201710687107A CN 107475552 A CN107475552 A CN 107475552A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0466—Alloys based on noble metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
Abstract
The invention provides the preparation method of silver-nickel material, comprise the following steps：A kind of preparation method of silver-nickel material, comprises the following steps：Prepare AgNO3, Ni (NO3) 2, Sm (NO3) 3, the mixed aqueous solutions of Sc (NO3) 3；Prepare excessive tetramethyl ammonium hydroxide solution；Under agitation, mixed solution is added drop-wise in tetramethyl ammonium hydroxide solution, generation is precipitated to reaction and finished；It is filtered under diminished pressure precipitation, precipitation is cleaned with deionized water, sediment decomposes in 300 DEG C of hydrogen atmospheres, reduces the nanoscale Ag, Ni for obtaining Dispersed precipitate, Sm, (Sc) powder；Powder sinters a pressing one-time sintering by 300MPa compactings, 700 DEG C of hydrogen atmospheres, and 500MPa compactings, 700 DEG C of hydrogen atmospheres sinter secondary compacting double sintering, are heated to 600 DEG C of extruding and AgNiSm (Sc) alloy material is prepared.Silver-nickel material prepared by the present invention will not introduce the impurity metallic elementses such as Na in preparation process, and preparation technology involved in the present invention is simple, the cycle is short, cost is low, suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of metal alloy compositions, more particularly to a kind of preparation side of silver-nickel material
Method.
Background technology
Silver nickel composite material (AgNi) contact resistance is low and stably, easy to process, and silver has good conduction and thermal conductivity
Can, nickel has good erosion-resisting characteristics, thus silver-colored nickel (AgNi) alloy material can obtain extensively in low capacity control apparatus
Using, it is the most frequently used contact material of contactor, relay, but material resistance fusion welding under high current is poor, in order to improve
The resistance fusion welding energy of material, researcher is usually added into rare earth material, while the Ni particles in material is refined, numerous studies and reality
Border application shows：In alloy material, more tiny Ni particles are more advantageous to improve resistance fusion welding energy, while it is also favourable to add rare earth
In the raising of resistance fusion welding energy.CN 10113966A disclose " a kind of preparation method of silver nickel composite material ", pass through preparation
Ag2NiO2 decomposition-reductions obtain scattered silver-colored nickel composite powder, then obtain micron-sized silver-nickel through oversintering, make material property
It is improved, but impurity Na ions is inevitably introduced in preparation process.
The content of the invention
It is an object of the invention to overcome the defect of prior art, there is provided a kind of preparation method of silver-nickel material,
It will not introduce the impurity metallic elementses such as Na in preparation process.
What the present invention was realized in：A kind of preparation method of silver-nickel material, comprises the following steps：
1) AgNO3, Ni (NO3) 2, Sm (NO3) 3, the mixed aqueous solutions of Sc (NO3) 3 are prepared；
2) excessive tetramethyl ammonium hydroxide solution is prepared；
3) under agitation, the mixed solution of step 1) is added drop-wise in the solution of step 2), generation is precipitated to reaction
Finish；
4) it is filtered under diminished pressure precipitation, cleans precipitation with deionized water, 2.5uS/cm is not higher than to filtrate electrical conductivity；
5) sediment decomposes in 300 DEG C of hydrogen atmospheres, reduces the nanoscale Ag, Ni for obtaining Dispersed precipitate, Sm, (Sc)
Powder；
6) powder sinters a pressing one-time sintering, 500MPa compactings, 700 by 300MPa compactings, 700 DEG C of hydrogen atmospheres
DEG C hydrogen atmosphere sinters secondary compacting double sintering, is heated to 600 DEG C of extruding and AgNiSm (Sc) alloy material is prepared.
Further, mixed solution concentration presses metal mass percent：Ag:Ni:Sm:(Sc)=88~89:10:1~2:
(0.5) AgNO3, Ni (NO3) 2, Sm (NO3) 3, the aqueous solution of Sc (NO3) 3, are mixed, in terms of AgNO3, AgNO3 solution is 0.20-
0.30mol/L。
Further, the precipitating reagent used is TMAH, concentration range 20%-30%.
Further, stirring condition is 1000~1300rmp of rotating speed.
Further, the alloy material being prepared is AgNiSm, AgNiSmSc.
The present invention provides a kind of preparation method of silver-nickel material, comprises the following steps：
1) AgNO3, Ni (NO3) 2, Sm (NO3) 3, the mixed aqueous solutions of Sc (NO3) 3 are prepared；By metal mass percent：Ag:
Ni:Sm:(Sc)=88~89:10:1~2:(0.5) AgNO3, Ni (NO3) 2, Sm (NO3) 3, the aqueous solution of Sc (NO3) 3, are mixed,
In terms of AgNO3, AgNO3 solution is 0.20-0.30mol/L；
2) excessive tetramethyl ammonium hydroxide solution is prepared；Concentration is 25%；
3) under agitation, the mixed solution of step 1) is added drop-wise in the solution of step 2), generation is precipitated to reaction
Finish；Low whipping speed is under 1000-1300rpm states, and the mixed solution of step 1 is added drop-wise in the solution of step 2, is added dropwise
Speed 2-3ml/S, generation are precipitated to reaction and finished, and PH is kept in course of reaction：11-13；
4) it is filtered under diminished pressure precipitation, cleans precipitation with deionized water, 2.5uS/cm is not higher than to filtrate electrical conductivity；
5) sediment decomposes in 300 DEG C of hydrogen atmospheres, reduces the nanoscale Ag, Ni for obtaining Dispersed precipitate, Sm, (Sc)
Powder；
6) powder sinters a pressing one-time sintering, 500MPa compactings, 700 by 300MPa compactings, 700 DEG C of hydrogen atmospheres
DEG C hydrogen atmosphere sinters secondary compacting double sintering, is heated to 600 DEG C of extruding and AgNiSm (Sc) alloy material is prepared.
Silver-nickel material prepared by the present invention will not introduce the impurity metallic elementses such as Na in preparation process, and
Preparation technology involved in the present invention is simple, the cycle is short, cost is low, suitable for industrialized production.
Embodiment
It is clearly and completely described below in conjunction with the technical scheme in the embodiment of the present invention, it is clear that described reality
It is only part of the embodiment of the present invention to apply example, rather than whole embodiments.It is general based on the embodiment in the present invention, this area
The every other embodiment that logical technical staff is obtained under the premise of creative work is not made, belong to what the present invention protected
Scope.
Embodiment one
Step 1：By metal mass percent：Ag:Ni:Sm=89:10:1, mixing AgNO3, Ni (NO3) 2, Sm (NO3) 3,
The aqueous solution of Sc (NO3) 3, in terms of AgNO3, AgNO3 solution is 0.20mol/L；
Step 2：Prepare excessive tetramethyl ammonium hydroxide solution, concentration 25%；
Low whipping speed is under 1000rpm states, and the mixed solution of step 1 is added drop-wise in the solution of step 2, and speed is added dropwise
2.4ml/s is spent, generation is precipitated to reaction and finished, and PH is kept in course of reaction：11-13；
It is filtered under diminished pressure precipitation, cleans precipitation with deionized water, 2.5uS/cm is not higher than to filtrate electrical conductivity；
Sediment decomposes in 300 DEG C of hydrogen atmospheres, reduces and obtains nanoscale Ag, Ni, Sm powder of Dispersed precipitate；
Powder sinters a pressing one-time sintering, 500MPa pressures by 300MPa compactings, 700 DEG C, 3 hours hydrogen atmospheres
System, 700 DEG C, the secondary compacting double sintering of hydrogen atmosphere sintering, are heated to 600 DEG C of extruding and AgNiSm (Sc) alloy material are prepared
Material.
Embodiment two
By metal mass percent：Ag:Ni:Sm:(Sc)=88:10:2:, mixing AgNO3, Ni (NO3) 2, Sm (NO3) 3
The aqueous solution, in terms of AgNO3, AgNO3 solution is 0.25mol/L；
Prepare excessive tetramethyl ammonium hydroxide solution, concentration 25%；
Low whipping speed is under 1200rpm states, and mixed solution is added drop-wise in tetramethyl ammonium hydroxide solution, and speed is added dropwise
2.5ml/S is spent, generation is precipitated to reaction and finished, and PH is kept in course of reaction：11-13；
It is filtered under diminished pressure precipitation, cleans precipitation with deionized water, 2.5uS/cm is not higher than to filtrate electrical conductivity；
Sediment decomposes in 300 DEG C of hydrogen atmospheres, reduces and obtains nanoscale Ag, Ni, Sm powder of Dispersed precipitate；
Powder sinters a pressing one-time sintering, 500MPa pressures by 300MPa compactings, 700 DEG C, 3 hours, hydrogen atmosphere
System, 700 DEG C, 3 hours secondary compacting double sinterings of hydrogen atmosphere sintering, are heated to 600 DEG C of extruding and AgNiSm alloys are prepared
Material.
Embodiment three
By metal mass percent：Ag:Ni:Sm:(Sc)=88.5:10:1:(0.5) AgNO3, Ni (NO3) 2, Sm, are mixed
(NO3) the 3, aqueous solution of Sc (NO3) 3, in terms of AgNO3, AgNO3 solution is 0.30mol/L；
Prepare excessive tetramethyl ammonium hydroxide solution, concentration 25%；
Low whipping speed is under 1300rpm states, and mixed solution is added drop-wise to tetramethyl ammonium hydroxide solution, rate of addition
2ml/s, generation are precipitated to reaction and finished, and PH is kept in course of reaction：11-13；
It is filtered under diminished pressure precipitation, cleans precipitation with deionized water, 2.5uS/cm is not higher than to filtrate electrical conductivity；
Sediment decomposes in 300 DEG C of hydrogen atmospheres, reduces and obtains nanoscale Ag, Ni, Sm, Sc powder of Dispersed precipitate；
Powder sinters a pressing one-time sintering, 500MPa pressures by 300MPa compactings, 700 DEG C, 3 hours hydrogen atmospheres
System, 700 DEG C, 3 hours secondary compacting double sinterings of hydrogen atmosphere sintering, are heated to 600 DEG C of extruding and AgNiSmSc conjunctions are prepared
Golden material.
Example IV
Step 1, by metal mass percent：Ag:Ni:Sm:(Sc)=87.5:10:2:0.5, mixing AgNO3, Ni (NO3)
2nd, Sm (NO3) 3, the aqueous solution of Sc (NO3) 3, in terms of AgNO3, AgNO3 solution is 0.25mol/L；
Step 2, excessive tetramethyl ammonium hydroxide solution, concentration 25% are prepared；
Low whipping speed is under 1100rpm states, and the mixed solution of step 1 is added drop-wise in the solution of step 2, and speed is added dropwise
2ml/S is spent, generation is precipitated to reaction and finished, and PH is kept in course of reaction：11-13；
It is filtered under diminished pressure precipitation, cleans precipitation with deionized water, 2.5uS/cm is not higher than to filtrate electrical conductivity；
Sediment decomposes in 300 DEG C of hydrogen atmospheres, reduces and obtains nanoscale Ag, Ni, Sm, Sc powder of Dispersed precipitate；
Powder sinters a pressing one-time sintering, 500MPa pressures by 300MPa compactings, 700 DEG C, 3 hours hydrogen atmospheres
System, 700 DEG C, 3 hours secondary compacting double sinterings of hydrogen atmosphere sintering, are heated to 600 DEG C of extruding and AgNiSmSc conjunctions are prepared
Golden material.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.
Claims (5)
1. a kind of preparation method of silver-nickel material, it is characterised in that comprise the following steps：
1) AgNO3, Ni (NO3) 2, Sm (NO3) 3, the mixed aqueous solutions of Sc (NO3) 3 are prepared；
2) excessive tetramethyl ammonium hydroxide solution is prepared；
3) under agitation, the mixed solution of step 1) is added drop-wise in the solution of step 2), generation is precipitated to reaction and finished；
4) it is filtered under diminished pressure precipitation, cleans precipitation with deionized water, 2.5uS/cm is not higher than to filtrate electrical conductivity；
5) sediment decomposes in 300 DEG C of hydrogen atmospheres, reduces the nanoscale Ag, Ni for obtaining Dispersed precipitate, Sm, (Sc) powder；
6) powder sinters a pressing one-time sintering, 500MPa compactings, 700 DEG C of hydrogen by 300MPa compactings, 700 DEG C of hydrogen atmospheres
The secondary compacting double sintering of gas atmosphere sintering, it is heated to 600 DEG C of extruding and AgNiSm (Sc) alloy material is prepared.
2. preparation method as claimed in claim 1, it is characterised in that：Mixed solution concentration presses metal mass percent：Ag:
Ni:Sm:(Sc)=88~89:10:1~2:(0.5) AgNO3, Ni (NO3) 2, Sm (NO3) 3, the aqueous solution of Sc (NO3) 3, are mixed,
In terms of AgNO3, AgNO3 solution is 0.20-0.30mol/L.
3. preparation method as claimed in claim 1, it is characterised in that：The precipitating reagent used is TMAH, concentration
Scope is 20%-30%.
4. preparation method as claimed in claim 1, it is characterised in that：Stirring condition is 1000~1300rmp of rotating speed.
5. preparation method as claimed in claim 1, it is characterised in that：The alloy material being prepared be AgNiSm,
AgNiSmSc。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710687107.1A CN107475552A (en) | 2017-08-11 | 2017-08-11 | A kind of preparation method of silver-nickel material |
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| CN201710687107.1A CN107475552A (en) | 2017-08-11 | 2017-08-11 | A kind of preparation method of silver-nickel material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108411135A (en) * | 2018-02-02 | 2018-08-17 | 东北大学 | A kind of silver-magnesium-nickel alloys band（Piece）, silk material preparation method |
| CN110317968A (en) * | 2019-07-03 | 2019-10-11 | 中国地质大学（武汉） | A kind of jewellery anti-tarnishing silver alloy and preparation method thereof |
-
2017
- 2017-08-11 CN CN201710687107.1A patent/CN107475552A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108411135A (en) * | 2018-02-02 | 2018-08-17 | 东北大学 | A kind of silver-magnesium-nickel alloys band（Piece）, silk material preparation method |
| CN108411135B (en) * | 2018-02-02 | 2020-04-24 | 东北大学 | Preparation method of silver-magnesium-nickel alloy strip (sheet) and wire |
| CN110317968A (en) * | 2019-07-03 | 2019-10-11 | 中国地质大学（武汉） | A kind of jewellery anti-tarnishing silver alloy and preparation method thereof |
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Address after: 508, building 428, Bagualing Industrial Zone, 43 Bagua Road, Hualin community, Yuanling street, Futian District, Shenzhen City, Guangdong Province Applicant after: SHENZHEN KMT TECHNOLOGY Co.,Ltd. Applicant after: TAIXING JINPENG TECHNOLOGY Co.,Ltd. Address before: 1, 14 floor, China Phoenix Building, No. 2008 Shennan Avenue, Shenzhen, Guangdong 518000, Futian District Applicant before: SHENZHEN YUANSIDACHENG TECHNOLOGY Co.,Ltd. Applicant before: TAIXING JINPENG TECHNOLOGY Co.,Ltd. |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20171215 |